Process of making terpin hydrate.



UN ITE s'rarns agrnnr uric LUDW'IG HEINRICH REUTER, QF NEW YORK, N. Y.

PROCESS OF' MAKING TERPIN HYDRATE.

Specification of Letters Patent.

Application filed February 24, 1906. Serial No. 302.739.

- Patented a... s, 1907.

To all whom, it WI/(147, concern:

Be it known that I, LUDWIGHEINRIOH REU- TER, a subject of the King of Bavaria, and a resident of thecity of New York, borough of Brooklyn, in the county of Kings and State of New York, have invented a new and Improved Method of Making T'erpin Hydrate,

of which the following is afull, clear, and exhydrate was generally known and that method involved the use of alcohol, the pric of which is high.

The manufacturing process which is employed in Europe is the so-called; nitricacid-alcohol process, which when carried out for four or five days yields terpin-hydrate crystals up to twenty pe cent. of the oil of turpentine used. It is intended in this process to recover the alcohol left in the mother-liquors for free use; but from my personal experience I am of the opinion that not only is a large proportion of the alcohol lost, but also about" thirty percent. of the oil, and that the oil which is recovered is partially oxidized or otherwise chemically changed in such a way that it cannot be used over again for the same kind of an operation.

- It is the purpose of my invention not only tofind a substitute for the nitric-aoid-alchol process which on account of not involving the'use of alcohol can be carried out on a commercial basis in the United States, but also to im rove the method of manufacturing terpin by rate in such a manner that more of the material employed can be recovered, and

- therefore to provide a process which can be also used to advantage in those countries in which alcohol for commercial purposes is not subject to tax.

I have discovered that in the manufacture of terpin hydrate the use of alcohol can be dispensed with, and, furthermore, that the cheapest of all acids-namely, sulfuric acidgives the best results. I have foundalso ,the bottom of the vat.

that it is'not necessary to employ the costly regular oil or spirits of turpentine of the market, which has to be used in the old process, but that oil or spirits of turpentine can be used as well as discolored or otherwise damaged andimpure oil of turpentine found n the southern pine districts of this country. In place-of the alcohol heretofore employed I use sawdust or any other similar substance which-is able to absorb oil or aqueous liquids Without combining chemically therewith. It will be seen, therefore, that my new process involves the use of practically the cheapest raw and waste materials-as, for example, 011 of turpentine, sulfuric acid, and sawdust.

As an example of manufacture, I mix in suitable vats, say, one hundred and twentyfive gallons of spirits of turpentine, any sultable quantitysay three hundred and fiftyoundsof sawdust or any other absorbent inert substance of a similar character. .As

soon as the oil has been roperly absorbed by the sawdust or the like add about seventeen hundred and fifty pounds of a diluted sulfuric acid or, in fact, a proportionate quantity ofany other acid except nitric acid. The whole is then mixed until a. uniform mass is obtained and then macerated at ordinary temperature for three or four Weeks. During this time a remarkable change takes place. A large percentage of the 0il,usually from fifty to sixty per cent, is converted into terpin hydrate, and the sawdust isfilledall through with crystals of the same. In about four to six Weeks time a maximum of the oil is converted, and for the purpose of removing the terpin hydrateit is necessary first to sepe non-converted oil and acid as far as arate t both can be removed by 0 ening a faucet at T en the balanceof the acid is removed by washing the sawdust with small portions of Water at a'timc, and finally the non-converted oil still left in the mass is removed by distillation with live steam. Theremaining mass, containin now only sawdustand terpin hydrate, issu jected to the action of boiling water under pressure for the purpose of dlssolvin the terpin hydrate and extracting it from t e sawdust. The hot concentrated solution of tar-pin hydrate is filtered, and rapidly crystallizes upon coolingj I have found that the recovered spirits of turpentine, all of the sawdust, the acid which is used, and the water in which the materials are Washed can be used over again'for new operations, so that the final manufacturing cost-price amounts .to only about one-seventh of that ofthe article made from alcohol, nitric acid,- and the regular spirits of turpenprocess an important industry can be develtine of the market. In fact, I have e env found that sawdust after being used several tiines gives expurer article than when used the first time. Regularspirits of turpentine can also be used instead of the wood spirits.

oped in the United States which has heretofore been exclusively carried outin foreign coun tries. An important advantageof ltalso 1s that certain raw and waste products can be employed which have heretofore had to be' refined and imported. I

Having thus described my invention, I

elaim i in a porous inactive solid and reacting on the mixture with a dilute acid, inlx ng, and'allowin the mixture to stand.

process of making terpin hydrate.

, name to this specification in the consisting in absorbing spirits .of turpentine process of making terpinhydrate,

in sawdust, treating the'admixture with sulfurlo acid, and allowlng the whole to stand.

4. A process of making 'terpin hydrate,

consistmg 1n mixing spirits of turpentine, a

dilute acid and a porous inactive materialwhich absorbs liquids, macerating the mixture, removing the acid and non-converted oil, and extracting terpin hydratefrom the residue.

5. A process of manufacturing terpin hy-. 'drat'e, consisting in mixlng's irits of turpentine, dilute sulfuric acid am a" porous inactlve materlal, inaceratnig the mixture, removing the acid and non-converted 011, and

"extracting turpi'n hydrate from the residue.

In testimony. whereof I have signed my two subscribing witne'sses.-

p LUDWIG HEINRICH REUTER. Witnesses:

ALBERT. E. FAY, EVERARD B. MARsHALL.

presence of.

'. '3. A process of makinp terpin hydrate consisting in absorbing spir ts of turpentine 

